Indium(III) reacts with α-diketone bisphenylthiosemicarbazones derived from glyoxal, biacetyl and methylglyoxal to form 1:1 and 1:2 (In: reagent) complexes in acid and basic medium, respectively. The effect of experimental variables was studied in detail on the acid site, and a new method for the spectrophotometric determination of indium(III) with meth-ylglyoxal bis(4-phenyl-3-thiosemicarbazone) (MGBPT) is proposed. The yellow 1:1 In-MGBPT complex is formed at pH 3.5–6 in a solution containing a 60 % V/V of dimethylforrnamide. The nature of the complex (ε = 27,100 1 mol−1cm−1at 465 mm) and the effect of interferences were studied.